1. 浙江工业大学化学工程与材料学院
2. 浙江省检验检疫科学技术研究院
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付馨慰, 黄超群, 蒋沁婷, 等. 液相色谱-串联质谱法测定人参中申嗪霉素的残留[J]. 分析测试学报, 2014,33(10):1204-1208.
Determination of Phenazine-1-carboxylic Acid Residue in Ginseng by Liquid Chromatography-Tandem Mass Spectrometry[J]. 2014,33(10):1204-1208.
建立了液相色谱-电喷雾串联质谱测定人参中申嗪霉素残留量的分析方法。人参样品经水浸泡,乙腈提取,分散固相萃取净化,色谱分离后,采用ESI-MS/MS在正离子多反应监测(MRM)模式下进行检测,选择定量离子对为m/z 225.1/179.1,定性离子对为m/z 225.1/125.1,外标法定量。该方法对于人参中申嗪霉素的定量下限为0.01 mg/kg,在0.5~10 μg/L质量浓度范围内,峰面积与含量呈良好线性关系,相关系数大于0.99。对人参中申嗪霉素在0.01,0.02,0.10 mg/kg加标水平下的回收率为82%~100%,相对标准偏差均不大于6.8%。结果表明,该方法操作简单、快速,灵敏度和准确度高,可满足人参中申嗪霉素残留量的检测要求。
A liquid chromatography coupled with electrospray ionization tandem mass spectrometric(LC-MS/MS) method was developed for the determination of phenazine-1-carboxylic acid in ginseng.The ginseng samples were soaked with water,extracted with acetonitrile and cleaned up by dispersive solid phase extraction,separated by chromatography,then detected by MS/MS under multiple reaction monitoring(MRM) mode via positive electrospray ionization.The ion-pair of 225.1/179.1 was used for quantitative analysis,and the ion-pair of 225.1/125.1 was selected for qualitative analysis.The external standard method was used for the quantification analysis.The limit of quantitation(LOQ) of phenazine-1-carboxylic acid was 0.01 mg/kg.The standard calibration curve was linear in the range of 0.5-10 μg/L,with correlation coefficient more than 0.99.The recoveries of phenazine-1-carboxylic acid in ginseng were in the range of 82%-100% at three spiked levels of 0.01,0.02 and 0.10 mg/kg,with relative standard deviations(RSDs) not more than 6.8%.The result showed that the method was simple,rapid and highly sensitive,and could be applied in the determination of phenazine-1-carboxylic acid in ginseng.
液相色谱-串联质谱法申嗪霉素人参
liquid chromatography-tandem mass spectrometry(LC-MS/MS)phenazine-1-carboxylic acidginseng
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